Method of distilling liquids.



L. 0. SHERMAN.

METHOD OF DISTILLING LIQUIDS. APPLICATION FILED MAR. 18, 1909.

968,088. V Patented Aug. 23, 1910.

2 sums-sum 1'.

L. 0'.- SHERMAN. METHOD OF DISTILIQING LIQUIDS.

8 APPLICATION FILED 53.18, 1909.

-Patented Aug. 28,1910.

genus-sum 2.

l I W618i??? I :O M f- @QW.

5 arson QsHEEMAmoz criivnnaim, 6a

'Ibdtl whom it may concern.

, Be it known that I, LAr'roN O. SHnaisiAN, a citizen of the United States, residing at Cleveland, the-county .of Cuyahoga and State of Ohio, have 1nve'ntecl 'certain new and;useful Improvements in Methods of Distill ng L1quids,.of which the following is a specification.

'lhe object of this invention isithe prov sion of a method of distilling hydrocarbon oils and other volatile liquids under-conditions yielding from crude materials a dis-' tillate of high --homogeneous c lpurity and grade and nearly aracter. According, to the method-the liquid is heated, and the resulting vapors. are causedto impingeat high velocity vupon: a chemically inert filling or obstructive material, and the portions of the vapors therebycondensed are returned to the still and reheated therein, the condensation and reheating being repeated many tunes; the uncondensed portion of the vapor is withdrawn and condensed in t-heusual manner as a practically homogeneous distillate.

For a full understanding'of my invention reference is made to the accompanying drawings wherein- Figure 1 is a long tudinal sectional'view show ng a preferredform of apparatus forv carrying themethod into effect; and la Flg. 2

' is a )lau-view of the same. Fin. 3 is a. sectional View of a check valve.

In said drawings, 1 represents an 0 1 still of ordinary type in the usual furnace setting 2. Near one end of the still is a vapor pipe 3 leading upwardly to a. casing or drum, from the upper portion of which extends an outlet 5 for the vapors which esca e condensation in the-drum, this outlet eading to a condenser ofany suitable type. Within the casing 4 is an obstructive filling 6, preferably employed in connection with baffles 7, 8, so arranged as to provide a tortuous and restricted path for the vapors.

As illustrated, the casing 4 .is rovided with an interior, perforated. meta ring 9 surrounding the aperture of the vapor plpe 3, a layer of the filling material 6 being distributed over the bottom of the casing around the ring 9. -Upon this layer is laced a disk-sha ed plate 7, of slightly less iameter than t e interior of the casing, roviding a peripheral vapor passage. The filling material is distributed in a thin layer over this plate and covered by a disk 8,

i-arson for premiums mourns,

Specification! Lettersr uen'a :Paten'td Aug. 2 3, a pucaabn' fllediliaren 18, ms. scream. 'isaaso. a I

. forming a tighti'ointwith' the'periphery of the casing and aving a centralaperture. This arrangement is continued to -the top of the casing, the plain and perforated disks "alternating'with each other, and the ob 'structive material filling the interstices. There is thus provided a long and tortuous vapor path, in traversing-which the vapors impinge at high velocity and at high temperature upon the obstructive filling. A progressive condensation ofthe vapors occurs, and the condensed portions are returned to'the s'till through pipes 10, tapped into opposite-sides of the casing at 11 ust above each of the battle plates 8: each of these pi es is preferably provided with check va ves indicated at 12 to prevent the liquid in the still from being forced, by excess of pressure therein, into the casing. Thesevera-l pipes 10 terminate in a manifold or header 13, which conducts the condensed liquid into the still," at a point below the. level of the liquid therein. Obviously a check valve may be inserted in the manifold adjacent the still, instead of providing valves in the individual return-flow pipes; 'the'latter arrangement is however considered preferable inasmuch asit permits the resistance offered by the drum to the vapors .to'be' varied atwill. Thusby closing the valves in the lower pipes (by means of the screws '30), liquid may be permitted to accuinulate in the filling, and to further ohstruct the movement of the vapors. this liquid being prevented by the high velocity of the vapors from flowing back into the I i still through the vapor pipe 3.

The fillingauaterial which I prefer to use is chemically inert toward the vapors, in the sense that it is not capable of entering into combination with the sulfur or any other constituent thereof. It is possible however that it may exert a catalytic action in breaking down the unsaturated bodies, particularly after it has become to some ex tent coated with deposited carb0n.' My preferred filling material consists of pebbles graded between the sizes of three-eighths and three-fourths inch.

The practice of the method, assuming a hydrocarbon oil to be treated, is as follows.

The oil vapors pass into the lower portion of the casing 4 and traverse the same at high velocity, being partly condensed in. and imparting their heatv to the filling material. As the operation proceeds a. temperature I the provision of whereby meson-- .densed vapors are returned to the lower pors.

i it entirely-evaporate; leaving 0 A the a the residue remaining in the still isfound 0f the casing; the rate of fall' of temperature oil throug a on I mately seven .feet in heigftby five 'et,.six

inch,,-I'have foun temperature difierence' 7 between the bottom and.top"-o f the casing u a ,tlgrade or even more liter stages,-

a. u bodies whee gof mb ed T e rehe'ahng'as renderedo'highly-efiective by tion of the still and are thereby thorougbl commmgledwith the residual-body o oil,

gradient is established'from bottom to-top varying with the size of the cas ng, the character of the -fillin thecharacter of theliquid disti11ed,i and t e stage of the operation: For exam' 1e. in distilling -a hydroordruma PIOIi':

inches in diameter, ghrovided with thirty six belles and with a ing 'ofpebbles ded between three-e hths'andZ-threeourtlis whidiiaries 15.". 'eent' e in the earlystagesiofthe o ration .to -100: cen- "difierence '.of temperature increas ng' 'ration'proceeds and beprorimat y m ionate to' {the specificgra'vity and V int-'of the ltqmd'inthe s't ill.- 'Thisfgipi in gmperature results in'a etiona j'e ghich becomes more pi'onounced' r: trons-as; the point ."0 the msi 'nal .1n the'. fondensed in aid-returns to the still "and-is" there're- ,heatedand in-' w'apo'rizemfthia' reheating.

and 'vafizihaa tidn repeated-many and atrepetition being to its lioili ngmpoint, before they m t s vp It s foun in-practice that the operation a disa 'pearance of these-called the disti la'te being w and and practically free from bloom. This term used to designate'the fattydfirtlon of the product, which is not: volatil e presence of this grease is determin n ract ee by pouring some of the product to tested on a sheet of white writing paper. If the productisfreefrom grease,. no line of demarcation. between that portion of the sheet wh1ch has been moistened and that which has not. It is-further observed that the-capillarity ofthe distillate is largely in resulting 'in, a material particularly adapted for burning .with-vvicks. Thatase is destroyed and not merely se ais clearly evident-from the fact t' at the depos oeapae to contain less: grease than the residues from similar oils which have undergone distillation in ordinary stills. The distillate is also nearly homogeneous in character. The above characteristics of thedistillate have proven. highly valuable in practice for certain pur- .pmes, notablyxin its use asf'asubstitute for tufi entine .for all painting'purposes- I y 'the expression obstructive filling herein employed; I mean afilling .which y its obstructive effect upon the ontflowin'gvapors will servefto. increase the .vapor pressure in the still and hence the temperature -of the vapors themselves to an extent, sutlicient to eflecta substantial separation of and greasev as above described. I 1 im=-.- j. 1.1 .The me ed at distilling crude "hydra :arbon oila which "consists in heating the -oil 'in; a still causing the, soproduoed' oilvapor to.' .throug'h a' deep layer of a granular. chemically inert to the vapor l0 --aifi%oiiering such resistanltlaeto thepaa'sage e-vapor' aSItO raise -t e. va r pressure the .still. and the .temperlizure of [the issuing i'a'po'r to apoint above that due to .tht'a-. norm'al boiling pointpf the 011 andsufiicient to eliminate grease'and snlfuflreturnin "the liquidsresulting from eondensati on -o vapor in the filling to the liquid 'in' he still and beneath the surface thereof, ind eondensing'the vapor, whereby there is roduced'a'greaseless and sulfur-free distil ate, -2- The method of dist crude h dro- --.carbon oils, whichconsists-in eating t e oil in a-still,.causing the so-produeed oil vase:- tp-pass through a deep layer of a gran ar g chemically inert" to the vapor, and 'o enng such resistance to the passage of the vapor as to raise the va '1' pressure within the still and the temperature of the issuing vapor to a point'abov'e that due to the nor- 'mal boiling point of the oil nndsuflicient to. eliminate grease and sulfur and to cause itlon of carbon" on the inert filling, returning the liquids resulting from c'onden'sation of vapor in the filling to the liquid 10 in. the still and beneath the surface thereof,'- and condensing the vapor whereby there is produced a'greaseless an sulfur-free'dis- 'tillat'e. a

In te'stimonv whereof, -I afli'x my signature 11 in presence of two witnesses.

LAYTOX. 0. SHERMAN.

\Vitnesses;

Hoaa'no. Foam; 

